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A new method based on a light-gas gun has been proposed to synthesize Nb-Al alloys, and a recovery capsule has been investigated. The copper-coated sample is accessible after shock wave loading. In this paper, we successfully synthesize Nb-Al alloys, which are high-temperature structural materials. X-ray diffraction is employed to clarify the structural characteristics of compounds after impact, and the simulation of X-ray diffractions is employed to clarify the structure. In detail, tetragonal NbAl3 alloys certainly appeared in the recovery capsule; this alloy is considered to be best candidate.